US4243646A - Treatment of carbon fibre - Google Patents

Treatment of carbon fibre Download PDF

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Publication number
US4243646A
US4243646A US05/948,293 US94829378A US4243646A US 4243646 A US4243646 A US 4243646A US 94829378 A US94829378 A US 94829378A US 4243646 A US4243646 A US 4243646A
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US
United States
Prior art keywords
fibre
resin matrix
carbon fibre
fiber
functional groups
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US05/948,293
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English (en)
Inventor
David J. Lind
Valerie J. Coffey
Joyce Hallam
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rolls Royce PLC
Original Assignee
Rolls Royce PLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rolls Royce PLC filed Critical Rolls Royce PLC
Priority to US06/148,318 priority Critical patent/US4284535A/en
Application granted granted Critical
Publication of US4243646A publication Critical patent/US4243646A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon

Definitions

  • This invention relates to the treatment of carbon fibre and in particular to a method of treating the surface of carbon fibre.
  • Carbon fibre is conventionally produced by subjecting an organic polymer fibre to various conditions of temperature and atmosphere.
  • polyacrylonitrile fibre may be heated at a temperature in the range 200 to 300° C. in an oxidising atmosphere and subsequently heated at a temperature of at least 1000° C. in an inert atmosphere to give carbon fibre.
  • Carbon fibre which is so produced is characterised by high breaking strain and Youngs modulus. Indeed such fibres are commonly incorporated in a resin matrix to provide a composite material having both strength and lightness.
  • a method of treating carbon fibre comprises subjecting the fibre to a surface removal step in which the surface layer of the fibre is removed together with any flaws therein and subsequently subjecting the fibre to a surface deactivation step in which at least some of the functional groups on the surface of said fibre are either removed or rendered incapable of forming a chemical bond with a resin matrix material.
  • Deactivation of the fibre surface may be achieved in two ways; either at least some of the functional groups may be removed or they may be rendered incapable of forming a chemical bond with a resin matrix material.
  • the fibre may be heated in an atmosphere of nitrogen at a temperature of 530° C.
  • the functional groups may be prevented from reacting with a resin matrix by providing the fibre with a coating of a material which does not form any chemical bond with either the fibre or the resin matrix.
  • One such suitable material is polyethylene.
  • a 220 meter length tow of 3000 filament high strain carbon fibre obtained from Toray Industries was wound on to a stainless steel frame.
  • the frame was then placed in a bath containing concentrated nitric acid (SG 1.42 g/ml) at a temperature of 80° C. After being agitated for a period of nine hours, the nitric acid was allowed to cool to room temperature whereupon the frame was removed and the carbon fibre sequentially washed in water, 1:3 v/v 0.88 ammonium hydroxide/water mixture, water and finally acetone before being dried at 80° C.
  • concentrated nitric acid SG 1.42 g/ml
  • Sample 1 A length of tow of the nitric acid treated fibre was then divided into two portions designated Sample 1 and Sample 2.
  • Sample 1 was then pulled through a bath containing a 2% w/v solution of polyethylene (molecular weight 2000) in xylene. After removal from the bath, the tow was dried at a temperature of 125° C. to leave each fibre with a polyethylene coating. The two was then pulled through a bath containing 100 parts by weight of Ciba Geigy CY 179 epoxy resin and 11/4 parts by weight of Ciba Geigy HG 973 BF 3 .MEA hardener. The resin impregnated tow was then removed from the bath and cured by heating in tension at a temperature of 130° C. for 1/2 hour.
  • the fibre tow which had not been subjected to the polyethylene coating step was inferior in both load to failure and fibre breaking stress to the fibre tow which had been so coated.
  • Example 1 A tow of high strain carbon fibre similar to that used in Example 1 was subjected to the same nitric acid treatment described in Example 1.
  • the tow was then divided into two portions; designed Sample 3 and Sample 4.
  • Sample 3 was passed through a furnace heated at a temperature of 530° C. and containing an atmosphere of nitrogen. Both portions were then impregnated with an epoxy resin/hardener mixture as described in Example 1 and similarly tested on the Instron tensile testing machine. The results were as follows:

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Inorganic Fibers (AREA)
  • Chemical Treatment Of Fibers During Manufacturing Processes (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Reinforced Plastic Materials (AREA)
US05/948,293 1977-10-04 1978-08-29 Treatment of carbon fibre Expired - Lifetime US4243646A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US06/148,318 US4284535A (en) 1978-08-29 1980-05-09 Rubber composites suitable for tire sidewalls from hexadiene polymer

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB41140/77 1977-10-04
GB4114077 1977-10-04

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
US72848276A Continuation 1976-09-30 1976-09-30

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US06/148,318 Division US4284535A (en) 1978-08-29 1980-05-09 Rubber composites suitable for tire sidewalls from hexadiene polymer
US06/149,930 Division US4269876A (en) 1977-10-04 1980-05-14 Treatment of carbon fibre

Publications (1)

Publication Number Publication Date
US4243646A true US4243646A (en) 1981-01-06

Family

ID=10418294

Family Applications (1)

Application Number Title Priority Date Filing Date
US05/948,293 Expired - Lifetime US4243646A (en) 1977-10-04 1978-08-29 Treatment of carbon fibre

Country Status (2)

Country Link
US (1) US4243646A (enrdf_load_stackoverflow)
JP (1) JPS5459497A (enrdf_load_stackoverflow)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040202603A1 (en) * 1994-12-08 2004-10-14 Hyperion Catalysis International, Inc. Functionalized nanotubes

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5721521A (en) * 1980-07-14 1982-02-04 Mitsubishi Rayon Co Ltd Production of carbon fiber of high strength and elongation
JPS58214527A (ja) * 1982-06-08 1983-12-13 Toray Ind Inc 高強伸度炭素繊維束
JPS61245368A (ja) * 1985-04-23 1986-10-31 東レ株式会社 炭素繊維の処理方法
JPS621749A (ja) * 1985-06-28 1987-01-07 Toray Ind Inc 高強度複合材料用プリプレグ
JPS6236427A (ja) * 1985-08-12 1987-02-17 Toray Ind Inc 一方向炭素繊維強化高強度複合材料
JPH076131B2 (ja) * 1985-12-18 1995-01-30 東レ株式会社 超高強度炭素繊維の製造方法
JPS62149969A (ja) * 1985-12-25 1987-07-03 東レ株式会社 炭素繊維の処理法
JPS62149971A (ja) * 1985-12-25 1987-07-03 東レ株式会社 高強度炭素繊維の製造方法
JPS62149972A (ja) * 1985-12-25 1987-07-03 東レ株式会社 炭素繊維の処理方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1124807A (en) * 1964-11-06 1968-08-21 Zieren Chemiebau Gmbh Dr A Improvements in and relating to the manufacture of sulphuric acid
US3476703A (en) * 1967-02-21 1969-11-04 Nat Res Dev Treatment of carbon fibres and composite materials including such fibres
US3720536A (en) * 1970-06-18 1973-03-13 United Aircraft Corp Treatment of carbon fibers
US3964952A (en) * 1971-03-19 1976-06-22 Commissariat A L'energie Atomique Method of manufacture of composite materials consisting of carbon fibers and resin and materials manufactured in accordance with said method
US4009305A (en) * 1972-12-22 1977-02-22 Kureha Kagaku Kogyo Kabushiki Kaisha Process for the surface treatment of carbon fibers
US4073869A (en) * 1975-06-05 1978-02-14 Celanese Corporation Internal chemical modification of carbon fibers to yield a product of reduced electrical conductivity

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5542514B2 (enrdf_load_stackoverflow) * 1971-09-28 1980-10-31
JPS5848490B2 (ja) * 1975-09-17 1983-10-28 シヨウワコウキ カブシキガイシヤ サンセイガスニヨルチユウワホウホウ

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1124807A (en) * 1964-11-06 1968-08-21 Zieren Chemiebau Gmbh Dr A Improvements in and relating to the manufacture of sulphuric acid
US3476703A (en) * 1967-02-21 1969-11-04 Nat Res Dev Treatment of carbon fibres and composite materials including such fibres
US3720536A (en) * 1970-06-18 1973-03-13 United Aircraft Corp Treatment of carbon fibers
US3964952A (en) * 1971-03-19 1976-06-22 Commissariat A L'energie Atomique Method of manufacture of composite materials consisting of carbon fibers and resin and materials manufactured in accordance with said method
US4009305A (en) * 1972-12-22 1977-02-22 Kureha Kagaku Kogyo Kabushiki Kaisha Process for the surface treatment of carbon fibers
US4073869A (en) * 1975-06-05 1978-02-14 Celanese Corporation Internal chemical modification of carbon fibers to yield a product of reduced electrical conductivity

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040202603A1 (en) * 1994-12-08 2004-10-14 Hyperion Catalysis International, Inc. Functionalized nanotubes

Also Published As

Publication number Publication date
JPS6311468B2 (enrdf_load_stackoverflow) 1988-03-14
JPS5459497A (en) 1979-05-14

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